Device for development in thin-layer chromatography

ABSTRACT

A device for development in thin-layer chromatography comprising a solvent chamber, a support means, a plurality of horizontal bars and one or more plates for development. The plate is suspended with a support means which can be rise or fall, and the lower end of said plate is soaked in solvent when it has become completely saturated. This solvent chamber brings about a good result on the reproducible quality of Rf values in thin-layer chromatography.

United States Patent 1191 Takeshita DEVICE FOR DEVELOPMENT IN THIN-LAYERCHROMATOGRAPHY [76] Inventor: Ryuzo Takeshita, No. 5-4-1 1, KoenziMinami, Tokyo, Japan [22] Filed: June 25, 1971 [21] Appl. No.: 156,766

[52] US. Cl. 210/198 [51] Int. Cl. 801d 15/08 [58] Field of Search210/31 C, 198 C [56] References Cited UNITED STATES PATENTS 1451 Aug.14, 1973 Primary Examiner-John Adee Att0rneyDavid Toren et al.

[5 7] ABSTRACT A device for development in thin-layer chromatographycomprising a solvent chamber, a support means, a plurality of horizontalbars and one or more plates for development. The plate is suspended witha support means which can be rise or fall, and the lower end of saidplate is soaked in solvent when it has become completely saturated. Thissolvent chamber brings about a good result on the reproducible qualityof R, values in thin-layer chromatography.

3,342,333 9/1967 Geiss et al.... 210/198 0 3,341,017 9/1967 Powell210/198 c 5 Clams 4 Drawing Figures DEVICE FOR DEVELOPMENT IN THIN-LAYERCHROMATOGRAPHY This invention relates to a solvent chamber for thinlayerchromatography in accordance with a method of absorption and partitionanalysis, especially to a device wherein compounds can be developed inthe saturation of solvent vapor, and thereby precise analysis, thereproducible R, values were gotten, and the development was easilyoperated.

As for conventional chromatography, after a compound to be examined isgiven to a plate to which adsorbent has been coated, the plate is placedaslant in a chamber by the wall of the chamber, in which solvent hasbeen placed shallowly. If such an operation is conducted, the lower edgeof the plate is immersed in the solvent and the plate is developedbefore the solvent vapor has saturated in the chamber. Therefore, anysubstance to be examined moves briskly before the adsorbent on the platehas fully been equilibrated with the solvent vapor. As the result ofthis development, time required for the saturation by a size of thechamber in which the compound has been developed, and the R, valueobtained thereby is changeable.

In this invention, a plate for development is suspended with a devisedsupport means which can be raised and lowered, and whenever the solventin the chamber has become completely saturated, the lower edge of theplate is immersed into the solvent so that the reproducible R, valuesare always obtained.

Namely, this invention relates to a device for developing chromatoplatesin thin-layer chromatography which is equipped with a hight-adjustablesupport means. They are made of such material as stainlesssteel or somekinds of plastics, which is proof aginst acids, alkalines, and organicsolvents. To a lower part of the support means, some of horizontal barsare connected. Thus a plate for development is suspended from the bar sothat its lower edge can be contacted with or separated from a solventsystem in the chamber.

By using this devised means, the plate can be lowered into a solventwithout opening the cover of the chamber after saturation of solventvapor, and then develpment can be started. In the process ofdevelopment, the so-called edge effect" which is a phenomenone thatsolvent front is curved during development because of unsaturation ofchamber, does not occure. In addition, the development can be conductedwith a relation that migration distance of the compound is proportionalto that of the solvent. As the result, the R, value of any compound isobtained with excellent reproducibility.

In addition, as the plates can be suspended with clips from somehorizontal bars fixed up to the support means, a plurality of plates canbe used for development, and raised or lowered smoothly.

Furthermore, there are two advantages as follows from such suspendingsystem: (1) The lower edge of the plate can be immersed into the solventto a desired depth even on the condition in which a large quantity ofsolvent has been put in the chamber. Without exchanging the solvent inthe chamber as far as the constituent of the solvent does not change,thin-layer chromatography is performed to continue for the same purpose.(2) The bottom of the chamber used need not be flat.

The invention will be described hereinafter with reference to theannexed drawing, in which FIG. 1 is the front view of the mode of anembodiment of this invention.

FIG. 2 is the cross sectional view of FIG. 1.

. FIG. 3 is the cross sectional view of the second embodiment of thisinvention, and

FIG. 4 is the drawing of the patterns wherein the distance of movementof a substance is shown by the longitudinal axis and the distance ofpermeation of solvent is shown by the transversal axis.

As shown in FIGS. 1 and 2, the solvent chamber 10 is made of glass, andin the shape of a somewhat deep box whose top is opened; its edge 11 isfinished smooth so that its interior can be tightly shut with a cover12.

The cover 12 is very tight and the support means 13 which also serves asa knob is fixed up approximately at the center of the cover. Saidsupport means 13 is composed of a guide pipe 14 fixed, a rod 15 insertedthrough the interior of the guide pipe 14 and a nut 17 screwed up to thescrew part 16 of the rod 15.

As shown in FIG. 2, a lower part of the guide pipe 14 is screwed up, andfixed with two ring nuts 18 and 19 from inside and outside of the cover12, through a hole at the center of the cover.

The rod 15 is inserted through the interior of the guide pipe and can berised and lowered byturning a ring 17.

If necessary, a packing and other suitable sealing means may be put onthe top of the guide pipe in order that solvent vapor in the interior ofthe solvent chamber 10 may not leak out of the space between the top ofthe guide pipe and a lower part of the ring 17.

At the lower end of the rod 15 is formed a screw 26, which is screwed upto the screw hole of an arm 20, and the rod 15 is vertically equipped ata right angle to the arm 20. At two sides of the arm 20 there are made aplurality of (four shown in the drawing) screw holes at intervals in thehorizontal direction, and into each screw hole 22 there is fixed up ahorizontal bar 21, from which the plate 24 of development is suspendedby means of a clip 23. The horizontal bars 21 are supported in parallelwith one another. The support means, arm and horizontal bars are made ofa stainless steel or plastic materials that remain uneffected by severalorganic solvent, acids or alkali.

Furthermore, it is also sufficient that ordinary holes are made on thearm 20 instead of a plurality of screw holes and a horizontal bar isinserted through each of the ordinary holes. 7

There are different sizes of chromatoplates such as 5 X 10cm, 5 X 20cm,20 X 20cm etc., and the embodiments shown in FIG. 1 and 2 respectivelyshow a case in which each of two plates having the size of 20 X 20cm issuspended by means of each of two horizontal bars 21. Of course, it isalso possible that each of a required number of the plates havingdifferent sizes is suspended by means of each horizontal bar. However,as for plates having such a short length as the 5 x IOcm-type, it issufficient that the rod 15 in the support means is replaced by anenormous rod or one enlarged by'connecting some joints 25a and 25bhaving a screw 36 respectively which is conjugated to the lower part ofthe rod 15 as shown in FIG. 3 so that the rod may have a requiredlength.

Besides, if the equilibration of each horizontal bar is difficult tokeep only by the arm 20, it is sufficient that a guide member (notshown) having the same shape as that of the support arm 20, is insertedinto one end of each horizontal bar 21 and through the bar in order thatthe equilibration may be kept by regulating the distance between thehorizontal bars 21.

After a spot of a substance to be examined is applied to the plate fordevelopment 24, the plate is suspended from a horizontal bar 21 with theclip 23, and without immersing the plate into the solvent setinto thesolvent chamber 10, in which amount of solvent 30 necessary fordevelopment has been put into the solvent chamber in advance. After theequilibration of the plate with solvent vaporis completely achieved inthe chamber, the plate 24 for development is immersed into the solventchamber by turning and adjusting the nut 17 of the support means andthus developed with the solvent 30. The rod of the support means 13 ismade to rise, and the lower end of the plate 24 is kept from soaking inthe solvent 30 in the solvent chamber. Namely, as the lower end of theplate 24 is distant from the solvent, in this condition there is nomovement of any substance on the plate and development is not yet made.

As a cover 12 is put on the top of the solvent chamber, solvent vaporforms its saturation after a while. After observing this, an adjustingnut 17 of the support means is loosened and the rod is made to slidedownward so that the lower end of the developing plate 24 can be made tosoak in the liquid layer of the solvent 30. In this way, the developingdoesn't start till the developing plate 24 is made to fall and touch thesolvent liquid. At this time, any substance and the solvent move verybriskly, as vaporization of the solvent from the plate does not occurbecause of saturation of the chamber, and, in addition, as shown in athick line in FIG. 4, the distance of movement of the substance is inright proportion to the distance of permeation of the solvent, so that astraight-line for development curve of any substance is drawn.

As seen from FIG. 4, the development curve of a compound isstraight-line according to this invention, and especially at the initialstage of the development high precision can be obtained as compared witha conventional method. Two thin and dotted lines shown in FIG. 4, showcurves obtained when some compounds,

one of which was different from the above compound, had been developed.

Besides, in the embodiments of this invention, 1 described aboutthin-layer chromatography, and it is needless to say that this inventioncanbe applied to paper-chromatography too.

I claim:

1. A device for deveopment in thin-layer chromatography comprising asolvent container, an air tight cover for said container, said containerand cover defining an airtight chamber in which a quantity of liquidsolvent is disposed, said chamber above said liquid solvent beingsaturated with said solvent, support means mounted on said cover andextending into said chamber, said support means suspending at least onedeveloping plate within said solvent chamber, and actuating meansoperatively connected to said support means and actuable externally ofsaid solvent chamber for raising and lowering said support means withinsaid chamber, whereby said developing plate is subjected to thesaturated solvent within said chamber above said quantity of liquidsolvent before being lowered for immersion into said liquid solvent.

2. Apparatus according to claim 1 wherein said cover has an opening,said support means comprising a guide tube mounted in said opening, arod mounted in said guide tube, a rotary element disposed externally ofsaid cover and operably with said rod to raise and lower the latter, andsupport elements within. said enclosure mounted on said rod for holdingsaid developing plate in a suspended disposition, whereby rotation ofsaid externally mounted rotary element lowers said development plate.

3. Apparatus according to claim 2 wherein said rod is provided withextension means, said support elements being mounted on said extensionmeans, thereby adapting said apparatus for handling shorter developingplates.

4. Apparatus according to claim 2 wherein clips are provided on saidsupport elements, said development plates being suspended by said clips.

5. Apparatus according to claim 4 wherein said clips are made ofpolyacetal resin.

patent 3,752, 316 Dated August 14, 1973 Inventor(s) Ryuzo hlta It iscertified that error appears in the above-identified patent and thatsaid Letters Patent are hereby corrected as shown below:

In the heading of the patent, the address of the inventor should read:

-No. 5-4-11, Koenji Minami, SuginaQmi-ku,

Tokyo, Japan-.

Signed and sealed this 23rd day of April 1971],.

(SEAL) Attest:

EDI-IARD PLFLETCHEILJR. C MARSHALL DAMN Attesting Officer Commissionerof Patents ORM PO-105O (10-69) usco M-Dc 60376-P69 w u. s. aovsmmzm'rnm'nua OFFICE 1 I!" o-aee-azu,

1. A device for deveopment in thin-layer chromatography comprising asolvent container, an air tight cover for said container, said containerand cover defining an airtight chamber in which a quantity of liquidsolvent is disposed, said chamber above said liquid solvent beingsaturated with said solvent, support means mounted on said cover andextending into said chamber, said support means suspending at least onedeveloping plate within said solvent chamber, and actuating meansoperatively connected to said support means and actuable externally ofsaid solvent chamber for raising and lowering said support means withinsaid chamber, whereby said developing plate is subjected to thesaturated solvent within said chamber above said quantity of liquidsolvent before being lowered for immersion into said liquid solvent. 2.Apparatus according to claim 1 wherein said cover has an opening, saidsupport means comprising a guide tube mounted in said opening, a rodmounted in said guide tube, a rotary element disposed externally of saidcover and operably with said rod to raise and lower the latter, andsupport elements within said enclosure mounted on said rod for holdingsaid developing plate in a suspended disposition, whereby rotation ofsaid externally mounted rotary element lowers said development plate. 3.Apparatus according to claim 2 wherein said rod is provided withextension means, said support elements being mounted on said extensionmeans, thereby adapting said apparatus for handling shorter developingplates.
 4. Apparatus according to claim 2 wherein clips are provided onsaid support elements, said development plates being suspended by saidclips.
 5. Apparatus according to claim 4 wherein said clips are made ofpolyacetal resin.